2-Nitroresorcinol synthesis
- Product Name:2-Nitroresorcinol
- CAS Number:601-89-8
- Molecular formula:C6H5NO4
- Molecular Weight:155.11
Yield: 27.4% ， 23.5%
Reaction Conditions:
with dihydrogen peroxide;sodium nitrite in aq. phosphate buffer; pH=7 at 20; for 1.58 h;Green chemistry;Reagent/catalyst;Concentration;
Steps:
9
At room temperature, 1 mmol of resorcinol was dissolved in 40 mL of phosphate buffer at pH = 7,Then, 60 mmol of sodium nitrite was added and 4 mmol of hydrogen peroxide was dissolved in 10 mL of phosphate buffer,in15 min into the reaction solution, at room temperature by adding 0.06g Fe-Al-MCM-41 molecular sieve to start the reaction, stirring reaction 80min. The filtrate was extracted with ethyl acetate (2 x 80 mL), concentrated under reduced pressure,Column chromatography (column packed with silica gel, eluted with petroleum ether and acetone as eluent,Petroleum ether and acetone volume ratio of 1: 1, that is, the target product 2 - nitroresorcinol, the yield of 27.4%And 4 - nitroresorcinol, the yield was 23.5% and the total yield was 50.9%. Under the same conditions,In the absence of the use of molecular sieve but 0.06gThe reaction was initiated using a water-soluble tetrakis (sodium sulfonate-based) iron porphyrin.As a result, the yield of 2-nitroresorcin was 9.9%, the yield of 4-nitroresorcin was 11.8%, The total yield was 21.7%.
References:
Qingdao Institute of Biomass Energy and Bioprocess Technology, Chinese Academy of Sciences;SUN, Wei-zhi;XU, Chao;XIAN, Mo;LIU, Fusheng;LIU, Yao-jie CN106045803, 2016, A Location in patent:Paragraph 0045-0046
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